HRID465254

反应详情

EQUATION

反应方程式

HRID 465254 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 50 ml of methylene chloride is dissolved 19 g of methyl 2-hydroxyiminoacetoacetate and under ice-cooling and stirring 19.6 g of sulfuryl chloride is added dropwise. The mixture is stirred at room temperature for 3 days, after which the methylene chloride is distilled off under reduced pressure. The residue is dissolved in 200 ml of ether and washed seven times with 100 ml portions of water. The ether layer is dried over anhydrous sodium sulfate and concentrated under reduced pressure to give 20.2 g of methyl 4-chloro-2-hydroxyiminoacetoacetate as a light-yellow oil.

WORKUP

后处理

  1. temperatureunder ice-cooling
  2. additionis added dropwise
  3. distillationafter which the methylene chloride is distilled off under reduced pressure
  4. dissolutionThe residue is dissolved in 200 ml of ether
  5. washwashed seven times with 100 ml portions of water
  6. dry with materialThe ether layer is dried over anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure